CN107357108A - Flexible glass electrochromism device and preparation method thereof - Google Patents
Flexible glass electrochromism device and preparation method thereof Download PDFInfo
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- CN107357108A CN107357108A CN201710590214.2A CN201710590214A CN107357108A CN 107357108 A CN107357108 A CN 107357108A CN 201710590214 A CN201710590214 A CN 201710590214A CN 107357108 A CN107357108 A CN 107357108A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/1533—Constructional details structural features not otherwise provided for
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- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
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Abstract
The invention discloses a kind of flexible glass electrochromism device and preparation method thereof, especially a kind of flexible glass GZO/PdCu/GZO (GPCG) structure P3HT film electrochromism devices and preparation method thereof, flexible GZO/PdCu/GZO plural layers are made by continuous volume to volume (R2R) method on the glass of flexible, and electrochromism device is prepared into using blade blade coating P3HT.The sheet resistance of GZO/PdCu/GZO structural membranes is 15 ohms/squares；Light transmittance 80%.Compared with individual layer GZO/P3HT, the GZO/PdCu/GZO/P3HT film electrochromism device coloring response time is short, stable performance.
Description
Technical field
The present invention relates to a kind of film electrochromism device, particularly a kind of flexible glass P3HT film electrochromism
Device and preparation method thereof.
Background technology
Flexible electronic is exactly the emerging electricity being produced on electronic device on flexible Drawability plastics, glass or thin metal matrix plate
Sub- technology, with its unique flexibility, ductility and efficient, inexpensive manufacturing process, led in information, the energy, medical treatment, national defence etc.
Domain has wide application prospect, such as flexible electronic displays, thin-film solar cell panel, electronics surface mount.Flexible electrical
Son have it is soft, deformable, light, portable, can the characteristic such as large-area applications, and by widely applying new material and new technology to produce
A large amount of new opplications are born, including RFID, Flexible Displays, OLED are luminous, sensor, flexible photovoltaic, logical AND store, flexible electrical
Pond.In future, " electronics paster " is pasted on the back of the hand with regard to that can detect ultraviolet degree of illumination；Pacemaker no longer changes electricity
Pond；Battery can directly wind production simultaneously.In recent years, this new branch of science of flexible electronic has caused domestic and international scientific and technological circle
With the extensive concern of industrial quarters, the R＆D process that numerous companies put into this sciemtifec and technical sphere is attract, accelerates flexible electrical
The practical product exploitation of son and commercialization process.Development in science and technology " 13 " planning in, country by policy guide with
Nursery finance will promote the flexible research and industrialization with printed electronic of China energetically.China is electronic industry big country, but is not
Technology is made the country prosperous, and flexible electronic is the chance that China strives for electronic industry great-leap-forward development.Flexible electronic has broad mass market, market
Scale is expanded rapidly, can turn into national pillar industry.
Flexible electronic transparent conductive film is exactly that caused film is not only conductive with more the transparency, is flexible
Thin film solar, display screen, electrochromic device, thin film transistor (TFT), electric capacity and electric resistance touch screen, transparent heater etc. it is important
Material.Compared with rigid substrate transparent conductive film, it also with flexibility and may extend away in addition to the conductive and transparency
Property, it is the important materials for developing flexible electronic device.
Flexible electrochromism device cannot be only used for intelligent window, automobile rearview mirror, display, can also directly be worn on soldier
Carry out with it military false proof.
The content of the invention
Goal of the invention：There is provided a kind of flexible glass GZO/PdCu/GZO/P3HT structural membrane electrochromism devices and
Its preparation method, flexible GZO/ is made by continuous volume to volume (R2R) method especially on the glass of flexible
PdCu/GZO plural layers, and electrochromism device is prepared into using blade blade coating P3HT.
Technical scheme：A kind of flexible glass electrochromism device, set on the glass of flexible flexible
GPCG plural layers, i.e. GZO/PdCu/GZO films, and flexible glass, GPCG multilayers are caused using blade blade coating P3HT films
Film and P3HT films are integrated into electrochromism device.
The stack manner of GZO/PdCu/GZO films is the structure of similar sandwich, is Ga-doped zinc oxide layer up and down,
Centre is Pd films, and Cu films are deposited on Pd films.
Further, the sheet resistance of GPCG films is 15 ohms/squares；Light transmittance 80%.
A kind of preparation method of flexible glass electrochromism device, it is characterised in that：Comprise the following steps：
Flexible glass is heated to 200 DEG C of removing surface moistures by step 1. in vacuum chamber；Then pass to 450/
5SCCM flows Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
Step 2. is in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
Spend 1m/min Ga-doped zinc oxide GZO rotary target materials deposit thickness 45nm in flexible glass film；
Step 3. arrives 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr in dc power 0.1；Flexible glass is wound
Speed 1m/mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；
Step 4. arrives 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr in dc power 0.1；Flexible glass is wound
Speed 1m/mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；
Step 5. repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, form GZO/
PdCu/GZO structural membranes；
Step 6. carries out structural characterization, with Hall measuring instruments, UV-Vis spectrometers, and XRD diffractometers, flexural measurement instrument, four
Probe resistance measuring instrument etc. measures to GZO/PdCu/GZO sheet resistance, light transmittance, structure and flexibility etc.；
Step 7. cleans up GZO/PdCu/GZO films with deionized water, in its surface blade blade coating P3HT electrochromism
Layer, then covers corresponding GZO/PdCu/GZO/ flexible glass and is prepared into electrochromism device；
Step 8. measures prepared electrochromism device.
Further, in the step 3, in dc power 0.1kW, Ar flow 300SCCM, operating pressure 2mTorr；It is soft
Property glass winding speed 1m/mi, Pd films are deposited with Pd planar targets on flexible glass GZO films；Meanwhile in step 4,
Dc power 0.1kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, with Cu planar targets
Cu films are deposited on flexible glass Pd films.
Further, in the step 3, in dc power 0.2kW, Ar flow 300SCCM, operating pressure 2mTorr；It is soft
Property glass winding speed 1m/mi, Pd films are deposited with Pd planar targets on flexible glass GZO films；Meanwhile in step 4,
Dc power 0.2kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, with Cu planar targets
Cu films are deposited on flexible glass Pd films.
Further, in the step 3, in dc power 0.3kW, Ar flow 300SCCM, operating pressure 2mTorr；It is soft
Property glass winding speed 1m/mi, Pd films are deposited with Pd planar targets on flexible glass GZO films；Meanwhile in step 4,
In dc power 0.3kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, with Cu flat targets
Material deposits Cu films on flexible glass Pd films.
Further, in the step 3, in dc power 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr；It is soft
Property glass winding speed 1m/mi, Pd films are deposited with Pd planar targets on flexible glass GZO films；Meanwhile in step 4,
In dc power 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, with Cu flat targets
Material deposits Cu films on flexible glass Pd films.
Beneficial effect：The present invention is compared with prior art：
(1) flexible glass electrochromism device is directly formed, can be used as " electronics paster ".
(2) the electric flexible glass electrochromism device formed；Performance is suitable with the performance of nonbreakable glass electrochromism device.
(3) flexible transparent electrode of R2R magnetron sputterings atomic deposition, reproducible, the electrochromism of highly reliable preparation
The device coloring response time is short, service life length.
(4) this method is applied to the production of large area flexible film electrochromism device, and speed is fast, high yield rate.
Brief description of the drawings
Fig. 1 is the structural representation of electrochromism device of the present invention.
1 in figure, flexible glass, 2, GPCG films, 3, P3HT films
Embodiment
A kind of large area flexible glass electrochromism device of the present invention and preparation method thereof step is as follows：
Flexible glass is heated to 200 DEG C of removing surface moistures by step 1. in vacuum chamber；Then pass to 450/
5SCCM flows Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
Step 2. is in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
Spend 1m/min Ga-doped zinc oxide (GZO) rotary target material deposit thickness 45nm in flexible glass film；
Step 3. arrives 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr in dc power 0.1；Flexible glass is wound
Speed 1m/mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；
Step 4. arrives 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr in dc power 0.1；Flexible glass is wound
Speed 1m/mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；
Step 5. repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, form GZO/
PdCu/GZO structural membranes；
Step 6. carries out structural characterization.With Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four
Probe resistance measuring instrument etc. measures to GZO/PdCu/GZO sheet resistance, light transmittance, structure and flexibility etc.；
Step 7. cleans up GZO/PdCu/GZO films with deionized water, in its surface blade blade coating P3HT electrochromism
Layer, then covers corresponding GZO/PdCu/GZO/ flexible glass and is prepared into electrochromism device.
Step 8. measures prepared electrochromism device.
Embodiment 1
(1) flexible glass is heated to 200 DEG C of removing surface moistures in vacuum chamber；Then pass to 450/5SCCM
Flow Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
(2) in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
1m/min, with Ga-doped zinc oxide (GZO) rotary target material deposit thickness 45nm in flexible glass film；
(3) in dc power 0.1kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；
(4) in dc power 0.1kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；
(5) repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, GZO/PdCu/ is formed
GZO structural membranes；
(6) structural characterization is carried out.With Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four probes
Resistance measuring instrument etc. measures to GZO/PdCu/GZO sheet resistance, light transmittance, structure and flexibility etc.；
(7) GZO/PdCu/GZO films are cleaned up with deionized water, P3HT electrochromic layers are scratched in its surface blade,
Then cover corresponding GZO/PdCu/GZO/ flexible glass and be prepared into electrochromism device.
(8) the prepared electrochromism device of measurement.
Embodiment 2
(1) flexible glass is heated to 200 DEG C of removing surface moistures in vacuum chamber；Then pass to 450/5SCCM
Flow Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
(2) in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
1m/min, with Ga-doped zinc oxide (GZO) rotary target material deposit thickness 45nm in flexible glass film；
(3) in dc power 0.2kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；
(4) in dc power 0.2kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；
(5) repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, GZO/PdCu/ is formed
GZO structural membranes；
(6) structural characterization is carried out.With Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four probes
Resistance measuring instrument etc. measures to ACA sheet resistance, light transmittance, structure and flexibility etc.；
(7) GZO/PdCu/GZO films are cleaned up with deionized water, P3HT electrochromic layers are scratched in its surface blade,
Then cover corresponding GZO/PdCu/GZO/ flexible glass and be prepared into electrochromism device.
(8) the prepared electrochromism device of measurement.
Embodiment 3
(1) flexible glass is heated to 200 DEG C of removing surface moistures in vacuum chamber；Then pass to 450/5SCCM
Flow Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
(2) in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
1m/min, with Ga-doped zinc oxide (GZO) rotary target material deposit thickness 45nm in flexible glass film；
(3) in dc power 0.3kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；
(4) in dc power 0.3kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；
(5) repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, GZO/PdCu/ is formed
GZO structural membranes；
(6) structural characterization is carried out.With Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four probes
Resistance measuring instrument etc. measures to ACA sheet resistance, light transmittance, structure and flexibility etc.；
(7) GZO/PdCu/GZO films are cleaned up with deionized water, P3HT electrochromic layers are scratched in its surface blade,
Then cover corresponding GZO/PdCu/GZO/ flexible glass and be prepared into electrochromism device.
(8) the prepared electrochromism device of measurement.
Embodiment 4
(1) flexible glass is heated to 200 DEG C of removing surface moistures in vacuum chamber；Then pass to 450/5SCCM
Flow Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
(2) in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
1m/min, with Ga-doped zinc oxide (GZO) rotary target material deposit thickness 45nm in flexible glass film；
(3) in dc power 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；
(4) in dc power 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/
Mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；
(5) repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, GZO/PdCu/ is formed
GZO structural membranes；
(6) structural characterization is carried out.With Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four probes
Resistance measuring instrument etc. measures to ACA sheet resistance, light transmittance, structure and flexibility etc.；
(7) GZO/PdCu/GZO films are cleaned up with deionized water, P3HT electrochromic layers are scratched in its surface blade,
Then cover corresponding GZO/PdCu/GZO/ flexible glass and be prepared into electrochromism device.
(8) the prepared electrochromism device of measurement.
Embodiment 5
(1) flexible glass is heated to 200 DEG C of removing surface moistures in vacuum chamber；Then pass to 450/5SCCM
Flow Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；
(2) in dc power 4.0kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed
1m/min, with Ga-doped zinc oxide (GZO) rotary target material deposit thickness 96nm in flexible glass film；
(3) structural characterization is carried out.With Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four probes
Resistance measuring instrument etc. measures to ACA sheet resistance, light transmittance, structure and flexibility etc.；
(4) GZO films are cleaned up with deionized water, in its surface blade blade coating P3HT electrochromic layer, then covered
Corresponding GZO flexible glass is prepared into electrochromism device.
(5) the prepared electrochromism device of measurement.
The flexible and transparent glass GPCG Structural Performance Analysis results of table 1
The flexible and transparent glass GPCG/P3HT of table 2 and GZO/P3HT film electrochromism device performance comparisions
Above-described embodiment is merely to illustrate the present invention, and according to above-described embodiment, the present invention may be better understood, and does not have to
In limitation the scope of the present invention.In addition, this area scientific research technical staff read the present invention after, with equivalent substitution or variable etc. pair
The present invention carries out various modifications, also belongs to claims of the present invention limited range.
Claims (7)
- A kind of 1. flexible glass electrochromism device, it is characterised in that：Set on the glass of flexible flexible GPCG plural layers, i.e. GZO/PdCu/GZO films, and flexible glass, GPCG multilayers are caused using blade blade coating P3HT films Film and P3HT films are integrated into electrochromism device.
- 2. flexible glass electrochromism device according to claim 1, it is characterised in that：The sheet resistance of GPCG films is 15 ohms/squares；Light transmittance 80%.
- A kind of 3. preparation method of flexible glass electrochromism device as claimed in claim 1, it is characterised in that：Including Following steps：Flexible glass is heated to 200 DEG C of removing surface moistures by step 1. in vacuum chamber；Then pass to 450/5SCCM streams Measure Ar/O2Surface plasma pretreatment cleaning is carried out under 600W DC voltages；Step 2. is in dc power 1.8kW, Ar/O2Flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/ Min Ga-doped zinc oxide GZO rotary target materials deposit thickness 45nm in flexible glass film；Step 3. arrives 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr in dc power 0.1；Flexible glass winding speed 1m/mi, Pd films are deposited on flexible glass GZO films with Pd planar targets；Step 4. arrives 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr in dc power 0.1；Flexible glass winding speed 1m/mi, Cu films are deposited on flexible glass Pd films with Cu planar targets；Step 5. repeat step (2), in Cu film surfaces deposition and the GZO films of step 2 same thickness, form GZO/PdCu/ GZO structural membranes；Step 6. carries out structural characterization, with Hall measuring instruments, UV-Vis spectrometers, XRD diffractometers, flexural measurement instrument, four probes Resistance measuring instrument etc. measures to GZO/PdCu/GZO sheet resistance, light transmittance, structure and flexibility etc.；Step 7. cleans up GZO/PdCu/GZO films with deionized water, and P3HT electrochromic layers are scratched in its surface blade, Then cover corresponding GZO/PdCu/GZO/ flexible glass and be prepared into electrochromism device；Step 8. measures prepared electrochromism device.
- 4. the preparation method of flexible glass electrochromism device according to claim 3, it is characterised in that：The step In rapid 3, in dc power 0.1kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, uses Pd Planar targets deposit Pd films on flexible glass GZO films；Meanwhile in step 4, in dc power 0.1kW, Ar flows 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, sunk with Cu planar targets on flexible glass Pd films Product Cu films.
- 5. the preparation method of flexible glass electrochromism device according to claim 3, it is characterised in that：The step In rapid 3, in dc power 0.2kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, uses Pd Planar targets deposit Pd films on flexible glass GZO films；Meanwhile in step 4, in dc power 0.2kW, Ar flows 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, sunk with Cu planar targets on flexible glass Pd films Product Cu films.
- 6. the preparation method of flexible glass electrochromism device according to claim 3, it is characterised in that：The step In rapid 3, in dc power 0.3kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, uses Pd Planar targets deposit Pd films on flexible glass GZO films；Meanwhile in step 4, in dc power 0.3kW, Ar flows 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, sunk with Cu planar targets on flexible glass Pd films Product Cu films.
- 7. the preparation method of flexible glass electrochromism device according to claim 3, it is characterised in that：The step In rapid 3, in dc power 0.4kW, Ar flow 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, uses Pd Planar targets deposit Pd films on flexible glass GZO films；Meanwhile in step 4, in dc power 0.4kW, Ar flows 300SCCM, operating pressure 2mTorr；Flexible glass winding speed 1m/mi, sunk with Cu planar targets on flexible glass Pd films Product Cu films.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109445220A (en) * | 2018-11-30 | 2019-03-08 | 东华大学 | A kind of spray coating method preparation large area P3HT base flexible electro-chromic device |
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| CN105845752A (en) * | 2016-04-04 | 2016-08-10 | 广州新视界光电科技有限公司 | Transparent conductive film applied to flexible photoelectric device and preparation method thereof |
| CN106024978A (en) * | 2016-06-16 | 2016-10-12 | 华东师范大学 | Transparent conductive thin film with metal alloy sandwich structure with anti-ultraviolet function |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09291355A (en) * | 1996-04-26 | 1997-11-11 | Asahi Glass Co Ltd | Transparent conductive film-provided substrate and its production |
| US20100079846A1 (en) * | 2005-07-01 | 2010-04-01 | Visiocorp Australia Pty Ltd | Charge conducting medium |
| CN103582844A (en) * | 2011-03-04 | 2014-02-12 | 纺织和塑料研究协会图林根研究院 | Stable electrochromic module |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109445220A (en) * | 2018-11-30 | 2019-03-08 | 东华大学 | A kind of spray coating method preparation large area P3HT base flexible electro-chromic device |
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